Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
2,6-Di-tert-butyl-4-methylpyridine → (S)-3-tert-Butoxycarbonylamino-4-methoxy-butyric acid benzyl ester
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 2,6-Di-tert-butyl-4-methylpyridine | HCID 98898 | — |
| 반응물 | Oxonium, trimethyl-, tetrafluoroborate(1-) (1:1) | HCID 2735153 | — |
| 반응물 | Phenylmethyl (3S)-3-[[(1,1-dimethylethoxy)carbonyl]amino]-4-hydroxybutanoate | HCID 10040985 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | (S)-3-tert-Butoxycarbonylamino-4-methoxy-butyric acid benzyl ester | HCID 57976545 | — |
반응 단계
To tert-butyl (S)-1-((benzyloxy)carbonyl)-3-hydroxypropan-2-ylcarbamate (1 eq.) in dichloromethane was added 2,6-di-t-butyl 4-methylpyridine (2.5 eq.) and trimethyloxonium tetrafluoroborate (1.25 eq.) at 0° C. The reaction mixture was gradually warm to room temperature and stirred overnight. The reaction mixture was diluted with dichloromethane and washed with cold satd. sodium bicarbonate, water, and brine and dried over sodium sulfate. Purification by silica gel chromatography (25% EtOAc/Hexane) provide pure product as a colorless viscous liquid.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07576221B2 |
| 출처 데이터셋 | uspto-grants-2009_08 |
| ORD ID | ord-f370348922ca4d1da77958c5dd1a6921 |
| 출처 메모 | uspto-grants-2009_08 |